Organic reactions in ionic liquids studied by in situ XPS.
Organic reactions in ionic liquids studied by in situ XPS.
复制标题
原位 XPS 研究离子液体中的有机反应。
作者：
Inga Niedermaier;C. Kolbeck;N. Taccardi;P. Schulz;Jing Li;T. Drewello;P. Wasserscheid;H. Steinrück;F. Maier
我们展示了原位 X 射线光电子能谱 (XPS) 在监测有机液相反应中的应用。通过将离子头基共价连接到反应有机分子上，可以降低它们的挥发性，从而使其能够承受超高真空条件。该方法对于有机反应的研究来说是一种新方法，可以在一个实验中以定量和氧化态敏感的方式跟踪反应混合物中存在的所有元素（氢除外）的命运。这一概念通过阴离子 4-氯丁基磺酸盐 ([ClC(4)H(8)SO(3)](-)) 对连接至咪唑鎓或鏻部分的叔胺进行烷基化得到了证明。在反应过程中，共价结合的氯转化为氯化物，胺转化为铵，这通过 N 1s 和 Cl 2p 结合能的明显变化反映出来。
We demonstrate the application of in situ X-ray photoelectron spectroscopy (XPS) to monitor organic, liquid-phase reactions. By covalently attaching ionic head groups to the reacting organic molecules, their volatility can be reduced such that they withstand ultra high vacuum conditions. The applied method, which is new for the investigation of organic reactions, allows for following the fate of all elements present in the reaction mixture--except for hydrogen--in a quantitative and oxidation-state-sensitive manner in one experiment. This concept is demonstrated for the alkylation of a tertiary amine attached to an imidazolium or phosphonium moiety by the anion 4-chlorobutylsulfonate ([ClC(4)H(8)SO(3)](-)). In the course of the reaction, the covalently bound chlorine is converted to chloride and the amine to ammonium as reflected by the distinct shifts in the N 1s and Cl 2p binding energies.